Antibacterial lyocell fiber and preparation method thereof

Abstract

The invention provides an antibacterial lyocell fiber and a preparation method thereof, and the preparation method of the lyocell fiber comprises the following steps: S1, adding a cinnamyl alcohol extract and alkylphenol polyoxyethylene ether into an ethanol / water mixed solvent to obtain an emulsion; s2, putting lyocell fibers into water to swell, washing and drying, dipping the lyocell fibers into the emulsion under the atmosphere of ultrasonic and protective gas, carrying out grafting reaction, washing and drying to obtain the antibacterial lyocell fibers. In the invention, water can generate free radicals under the action of ultrasonic irradiation, and the free radicals can initiate a grafting reaction, so that antibacterial active components such as cinnamic acid containing carbon-carbon double bonds, cinnamyl aldehyde and the like in the cinnamyl alcohol extract are combined to the fiber through chemical bonds, and the lyocell fiber is endowed with an antibacterial effect.

Description

Technical Field

[0001] This invention relates to the field of textile technology, and in particular to an antibacterial lyocell fiber and its preparation method. Background Technology

[0002] Lyocell fiber, also known as "Tencel," is a regenerated cellulose fiber made from natural plant pigments using an NMMO solvent spinning process. The raw material for lyocell fiber is pulp formed from the crushing of widely available and renewable natural resources such as bamboo and wood. No chemical reactions occur during the production process, and the NMMO solvent used in its preparation is non-toxic with a recovery rate of up to 99.7%, making it energy-saving, environmentally friendly, and sustainable. Lyocell fiber combines many excellent properties of both natural and synthetic fibers, possessing advantages such as high strength, high swelling capacity, good comfort, natural luster, smooth hand feel, high moisture absorption, good breathability, easy dyeing, and strong spinnability. It is widely used in textiles such as clothing, duvet covers, sheets, pillowcases, and fitted sheets.

[0003] In recent years, with the improvement of living standards, people's use of textiles is no longer limited to comfort. More and more users have put forward higher requirements for the function of textiles, such as hoping that textiles have antibacterial, cooling and health care effects.

[0004] However, Lyocell fibers are highly absorbent and have a high standard moisture regain. In humid environments, they can easily become a culture medium for pathogens such as bacteria and fungi. Long-term contact with fabrics that are not completely dried can increase the risk of skin infections and is detrimental to health.

[0005] In summary, there is an urgent need for a method to prepare antibacterial lyocell fibers in order to endow them with antibacterial properties. Summary of the Invention

[0006] This invention provides an antibacterial lyocell fiber and its preparation method, thereby endowing the lyocell fiber with antibacterial properties.

[0007] To achieve the above objectives, the technical solution of the present invention is as follows: In a first aspect, the present invention provides a method for preparing antibacterial lyocell fiber, the method comprising the following steps: S1. Add cinnamon extract and alkylphenol polyoxyethylene ether to an ethanol / water mixed solvent to obtain an emulsion; S2. After soaking and swelling the Lyocell fiber in water, wash and dry it. Then, immerse the Lyocell fiber in the emulsion under ultrasonic and protective gas atmosphere to carry out the grafting reaction. Wash and dry the fiber to obtain the antibacterial Lyocell fiber.

[0008] In one embodiment of the present invention, in the ethanol / water mixed solvent of step S1, the volume ratio of ethanol to water is 1:1-3, preferably 1:2-3.

[0009] In one embodiment of the present invention, in step S1, the mass ratio of the alkylphenol polyoxyethylene ether to the cinnamon alcohol extract is 0.002-0.005:1, preferably 0.003-0.005:1.

[0010] In one embodiment of the present invention, the concentration of the cinnamon alcohol extract in the emulsion in step S1 is 2-3 g / 100 mL, preferably 2.5-3 g / 100 mL.

[0011] In one embodiment of the present invention, carbon tetrachloride is also added to the emulsion in step S1.

[0012] In one embodiment of the present invention, in step S1, the mass ratio of carbon tetrachloride to cinnamyl alcohol extract is 0.3-0.6:1, preferably 0.4-0.6:1.

[0013] In one embodiment of the present invention, during the swelling process described in step S2, the bath ratio is 1:10-20, preferably 1:15-20.

[0014] In one embodiment of the present invention, in step S2, the frequency of the ultrasound is 10-18 kHz, preferably 12-18 kHz.

[0015] In one embodiment of the present invention, in step S2, the temperature of the grafting reaction is 25-30°C, preferably 27-30°C; and the time of the grafting reaction is 1-3 hours, preferably 1.5-3 hours.

[0016] In one embodiment of the present invention, in step S2, the drying temperature is 50-60°C, preferably 55-60°C; the drying time is 20-30 min, preferably 25-30 min.

[0017] Secondly, the present invention also provides an antibacterial lyocell fiber prepared according to the method described above.

[0018] As described above, the antibacterial lyocell fiber and its preparation method of the present invention have the following beneficial effects: In this invention, water can generate free radicals under ultrasonic irradiation. These free radicals can initiate a grafting reaction, allowing the antibacterial active ingredients such as cinnamic acid and cinnamaldehyde, which contain carbon-carbon double bonds, in the cinnamic alcohol extract to be chemically bonded to the fiber, thus giving the lyocell fiber antibacterial properties.

[0019] In this invention, volatile carbon tetrachloride can enter the cavitation bubbles generated by ultrasound to capture hydrogen free radicals, reduce the possibility of hydroxyl free radicals recombine with hydrogen free radicals to generate water, increase the content of hydroxyl free radicals in the emulsion, improve grafting efficiency, and further enhance the antibacterial effect of Lyocell fiber. Detailed Implementation

[0020] The following specific examples illustrate the implementation of the present invention. Those skilled in the art can easily understand other advantages and effects of the present invention from the content disclosed in this specification. The present invention can also be implemented or applied through other different specific embodiments. Various details in this specification can also be modified or changed based on different viewpoints and applications without departing from the spirit of the present invention. In the absence of conflict, the following embodiments and features in the embodiments can be combined with each other.

[0021] An embodiment of the present invention provides a method for preparing antibacterial lyocell fiber, the method comprising the following steps: S1. Add cinnamon extract and alkylphenol polyoxyethylene ether to an ethanol / water mixed solvent to obtain an emulsion; S2. After soaking and swelling the Lyocell fiber in water, wash and dry it. Then, immerse the Lyocell fiber in an emulsion under ultrasonic and protective gas atmosphere to carry out a grafting reaction. After washing and drying, antibacterial Lyocell fiber is obtained.

[0022] In this invention, water can generate free radicals under ultrasonic irradiation. These free radicals can initiate a grafting reaction, allowing the antibacterial active ingredients such as cinnamic acid and cinnamaldehyde, which contain carbon-carbon double bonds, in the cinnamic alcohol extract to be chemically bonded to the fiber, thus giving the lyocell fiber antibacterial properties.

[0023] In one embodiment of the present invention, in the ethanol / water mixed solvent of step S1, the volume ratio of ethanol to water is 1:1-3, preferably 1:2-3.

[0024] In one embodiment of the present invention, in step S1, the mass ratio of alkylphenol polyoxyethylene ether to cinnamon alcohol extract is 0.002-0.005:1, preferably 0.003-0.005:1. Examples of alkylphenol polyoxyethylene ethers include, for example, dodecylphenol polyoxyethylene ether (NP-10), nonylphenol polyoxyethylene ether (TX-10), and octylphenol polyoxyethylene ether (OP-10).

[0025] In one embodiment of the present invention, the concentration of cinnamon alcohol extract in the emulsion of step S1 is 2-3 g / 100 mL, preferably 2.5-3 g / 100 mL.

[0026] In one embodiment of the present invention, carbon tetrachloride is further added to the emulsion in step S1. The mass ratio of carbon tetrachloride to cinnamon alcohol extract is 0.3-0.6:1, preferably 0.4-0.6:1.

[0027] In this invention, volatile carbon tetrachloride can enter the cavitation bubbles generated by ultrasound to capture hydrogen free radicals, reduce the possibility of hydroxyl free radicals recombine with hydrogen free radicals to generate water, increase the content of hydroxyl free radicals in the emulsion, improve grafting efficiency, and further enhance the antibacterial effect of Lyocell fiber.

[0028] In one embodiment of the present invention, in step S2, during the swelling process, the bath ratio is 1:10-20, preferably 1:15-20. The swelling time is 1-2 hours, preferably 1.5-2 hours.

[0029] In one embodiment of the present invention, in step S2, the frequency of the ultrasound is 10-18 kHz, preferably 12-18 kHz.

[0030] In one embodiment of the present invention, in step S2, the temperature of the grafting reaction is 25-30°C, preferably 27-30°C; the time of the grafting reaction is 1-3 hours, preferably 1.5-3 hours.

[0031] In one embodiment of the present invention, in step S2, the drying temperature is 50-60°C, preferably 55-60°C; the drying time is 20-30 min, preferably 25-30 min.

[0032] Another embodiment of the present invention also provides an antibacterial lyocell fiber prepared according to the method described above.

[0033] The present invention will be described in detail below through specific examples and embodiments. It should also be understood that the following embodiments are only for specific illustration of the present invention and should not be construed as limiting the scope of protection of the present invention. Any non-essential improvements and adjustments made by those skilled in the art based on the above description of the present invention are within the scope of protection of the present invention. The specific process parameters, etc., in the following examples are merely examples within a suitable range; that is, those skilled in the art can make appropriate selections within the appropriate range based on the description herein, and are not intended to be limited to the specific values ​​in the examples below.

[0034] Example 1 A method for preparing antibacterial lyocell fiber, the specific steps of which are as follows: S1. Mix anhydrous ethanol and water at a volume ratio of 1:3 to obtain an ethanol / water mixed solvent; Cinnamyl alcohol extract (commercially available) and octylphenol polyoxyethylene ether (OP-10) were added to an ethanol / water mixed solvent to obtain an emulsion with a cinnamyl alcohol extract concentration of 3 g / 100 mL and a mass ratio of octylphenol polyoxyethylene ether to cinnamyl alcohol extract of 0.002:1. S2. Soak the Lyocell fiber in water for 1 hour, with a bath ratio of 1:20; Then wash and dry; Next, Lyocell fibers were impregnated in an emulsion under an ultrasonic and nitrogen atmosphere to carry out a grafting reaction at 25°C for 3 hours, with an ultrasonic frequency of 18kHz. Wash and then dry at 50°C for 30 minutes to obtain antibacterial lyocell fiber.

[0035] Example 2 A method for preparing antibacterial lyocell fiber, the specific steps of which are as follows: S1. Mix anhydrous ethanol and water at a volume ratio of 1:1 until homogeneous to obtain an ethanol / water mixed solvent; Cinnamyl alcohol extract (commercially available) and dodecylphenol polyoxyethylene ether (NP-10) were added to an ethanol / water mixed solvent to obtain an emulsion with a cinnamyl alcohol extract concentration of 2 g / 100 mL and a mass ratio of dodecylphenol polyoxyethylene ether to cinnamyl alcohol extract of 0.005:1. S2. Soak the Lyocell fiber in water for 2 hours to swell, with a bath ratio of 1:10; Then wash and dry; Next, the Lyocell fiber was impregnated in an emulsion under an ultrasonic and nitrogen atmosphere, and the grafting reaction was carried out at 30°C for 1 hour with an ultrasonic frequency of 10 kHz. Wash and then dry at 60°C for 20 minutes to obtain antibacterial lyocell fiber.

[0036] Example 3 A method for preparing antibacterial lyocell fiber, the specific steps of which are as follows: S1. Mix anhydrous ethanol and water at a volume ratio of 1:2 to obtain an ethanol / water mixed solvent; Cinnamyl alcohol extract (commercially available) and nonylphenol polyoxyethylene ether were added to an ethanol / water mixed solvent to obtain an emulsion with a concentration of 2.5 g / 100 mL of cinnamyl alcohol extract and a mass ratio of nonylphenol polyoxyethylene ether to cinnamyl alcohol extract of 0.003:1. S2. Soak the Lyocell fiber in water for 1.5 hours at a bath ratio of 1:15; Then wash and dry; Next, the Lyocell fiber was impregnated in an emulsion under an ultrasonic and nitrogen atmosphere, and the grafting reaction was carried out at 28°C for 2 hours with an ultrasonic frequency of 15kHz. Wash and then dry at 55°C for 25 minutes to obtain antibacterial lyocell fiber.

[0037] Example 4 The difference between this embodiment and embodiment 3 is as follows: S1. Mix anhydrous ethanol and water at a volume ratio of 1:2 to obtain an ethanol / water mixed solvent; Cinnamyl alcohol extract (commercially available), nonylphenol polyoxyethylene ether, and carbon tetrachloride were added to an ethanol / water mixed solvent to obtain an emulsion with a cinnamyl alcohol extract concentration of 2.5 g / 100 mL. The mass ratio of nonylphenol polyoxyethylene ether to cinnamyl alcohol extract was 0.003:1, and the mass ratio of carbon tetrachloride to cinnamyl alcohol extract was 0.3:1.

[0038] In this embodiment, carbon tetrachloride is also added to the emulsion, and the mass ratio of carbon tetrachloride to cinnamon alcohol extract is 0.3:1.

[0039] Example 5 The difference between this embodiment and embodiment 3 is as follows: S1. Mix anhydrous ethanol and water at a volume ratio of 1:2 to obtain an ethanol / water mixed solvent; Cinnamyl alcohol extract (commercially available), nonylphenol polyoxyethylene ether, and carbon tetrachloride were added to an ethanol / water mixed solvent to obtain an emulsion with a concentration of 2.5 g / 100 mL of cinnamyl alcohol extract. The mass ratio of nonylphenol polyoxyethylene ether to cinnamyl alcohol extract was 0.003:1, and the mass ratio of carbon tetrachloride to cinnamyl alcohol extract was 0.6:1.

[0040] In this embodiment, carbon tetrachloride is also added to the emulsion, and the mass ratio of carbon tetrachloride to cinnamon alcohol extract is 0.6:1.

[0041] Comparative Example 1 This comparative example uses Lyocell fibers from the same source as in Example 3.

[0042] Performance testing The antibacterial lyocell fibers obtained in Examples 1-5 and the lyocell fibers of Comparative Example 1 were processed into fabrics. The inhibitory values ​​of each fabric against Staphylococcus aureus (ATCC 6538) and Escherichia coli (ATCC 11229) were tested according to GB / T 20944.2-2007 Evaluation of antibacterial properties of textiles - Part 2: Absorption method. The test bacterial solutions were prepared after being cultured according to the C culture method. The results are shown in Table 1.

[0043] Table 1. Results of antibacterial performance test

[0044] As shown in Table 1, compared with Comparative Example 1 (without modification of lyocell fiber), the fabric processed from the antibacterial lyocell fiber of Example 3 (with modified lyocell fiber) showed significantly improved inhibitory values ​​against Staphylococcus aureus and Escherichia coli. This result indicates that in this invention, water under ultrasonic irradiation can generate free radicals, which can initiate a grafting reaction, causing the antibacterial active ingredients such as cinnamic acid and cinnamaldehyde containing carbon-carbon double bonds in the cinnamic alcohol extract to chemically bind to the fiber, thus endowing the lyocell fiber with antibacterial properties.

[0045] As shown in Table 1, compared with Example 3 (no carbon tetrachloride added to the emulsion), the fabrics processed from antibacterial lyocell fibers in Examples 4 (carbon tetrachloride added to the emulsion) and 5 (carbon tetrachloride added to the emulsion) showed significantly improved inhibitory values ​​against Staphylococcus aureus and Escherichia coli. This result indicates that, in this invention, volatile carbon tetrachloride can enter the cavitation bubbles generated by ultrasound to capture hydrogen free radicals, reducing the likelihood of hydroxyl radicals recombinating with hydrogen free radicals to generate water, increasing the content of hydroxyl radicals in the emulsion, improving grafting efficiency, and further enhancing the antibacterial effect of lyocell fibers.

[0046] The above embodiments are merely illustrative of the principles and effects of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or alter the above embodiments without departing from the spirit and scope of the present invention. Therefore, all equivalent modifications or alterations made by those skilled in the art without departing from the spirit and technical concept disclosed in the present invention should still be covered by the claims of the present invention.

Claims

1. A method for producing an antibacterial lyocell fiber, characterized by, The preparation method of the antibacterial lyocell fiber comprises the following steps: S1. Adding cinnamyl alcohol extract and alkyl phenol polyoxyethylene ether into an ethanol / water mixed solvent to obtain an emulsion; S2. After swelling the lyocell fiber in water, washing and drying, the lyocell fiber is immersed in the emulsion under ultrasonic and protective gas atmosphere to carry out grafting reaction, washing and drying to obtain the antibacterial lyocell fiber.

2. The method of producing an antibacterial lyocell fiber according to claim 1, characterized by, In the ethanol / water mixed solvent of step S1, the volume ratio of ethanol to water is 1:1-3.

3. The method of producing an antibacterial lyocell fiber according to claim 1, wherein In step S1, the mass ratio of the alkyl phenol polyoxyethylene ether to the cinnamyl alcohol extract is 0.002-0.005:

1.

4. The method of producing an antibacterial lyocell fiber according to claim 1, characterized by, In the emulsion of step S1, the concentration of the cinnamyl alcohol extract is 2-3g / 100mL.

5. The method of producing an antibacterial lyocell fiber according to claim 1, wherein Carbon tetrachloride is also added in the emulsion of step S1.

6. The method of producing an antibacterial lyocell fiber according to claim 5, characterized by, In step S1, the mass ratio of the carbon tetrachloride to the cinnamyl alcohol extract is 0.3-0.6:

1.

7. The method of producing an antibacterial lyocell fiber according to claim 1, wherein In the swelling process of step S2, the bath ratio is 1:10-20.

8. The method of producing an antibacterial lyocell fiber according to claim 1, wherein In step S2, the frequency of the ultrasonic is 10-18kHz; And / or, in step S2, the temperature of the grafting reaction is 25-30℃, and the time of the grafting reaction is 1-3h.

9. The method of producing an antibacterial lyocell fiber according to claim 1, wherein In step S2, the temperature of the drying is 50-60℃, and the time of the drying is 20-30min.

10. An antibacterial lyocell fiber prepared according to the method of any one of claims 1-9.

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